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Method for preparing poly-1,3-pentadiene

A technology of pentadiene and CF3SO3, applied in the field of catalyst and its preparation, can solve the problems of corrosion of polymerization equipment and harsh preparation conditions, and achieve the effects of eliminating corrosion, reducing preparation cost and simplifying process procedures

Inactive Publication Date: 2012-02-15
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI +1
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

At present, the rare earth sulfonate catalyst systems used in the polymerization of diolefins include rare earth chloride complexes and rare earth carboxylic acid catalysts. The rare earth chloride complexes are prepared under harsh conditions. In addition to the base aluminum, a third component needs to be added, and the third component is often a compound containing a chlorine source, which not only increases the cost of synthesizing poly-1,3-pentadiene, but also corrodes the polymerization equipment

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[0031] The present invention also provides a preparation method of a rare earth complex, a) mixing trifluoromethanesulfonic acid with a rare earth oxide, and reacting to obtain a rare earth trifluoromethanesulfonic acid compound;

[0032] b) The rare earth trifluoromethanesulfonic acid compound and the electron-donating ligand are mixed in a solvent, heated to boiling and then refluxed, and then the solvent is drained to obtain the rare earth trifluoromethanesulfonic acid complex Ln(CF 3 SO 3 ) 3 ·xH 2 O·yL; wherein, Ln is a trivalent cation of a rare earth element, L is an electron-donating ligand, 0<x≤6, 1≤y≤4.

[0033] And a kind of preparation method of catalyst for 1,3-pentadiene polymerization, comprising

[0034] The molar ratio is (20-60): 1, the alkylaluminum and the trifluoromethanesulfonate rare earth complex are mixed, and aged in hexane to obtain a catalyst for the polymerization of piperylene.

[0035] There is also a preparation method of poly-1,3-pentadiene, ...

Embodiment 1

[0049] Preparation of Neodymium Trifluoromethanesulfonate

[0050] In the reactor, according to the molar ratio of neodymium oxide and trifluoromethanesulfonic acid, neodymium oxide is added to the trifluoromethanesulfonic acid solution at a ratio of 10:1, heated to 70° C. under stirring conditions, reacted for 8 hours, filtered, and The unreacted neodymium oxide is removed, the aqueous solution of neodymium trifluoromethanesulfonate is concentrated, and then the concentrated aqueous solution of neodymium trifluoromethanesulfonate is placed at room temperature to naturally precipitate crystals, which is neodymium trifluoromethanesulfonate with crystal water.

Embodiment 2

[0052] Preparation of Lanthanum Trifluoromethanesulfonate

[0053] In the reactor, according to the molar ratio of lanthanum oxide and trifluoromethanesulfonic acid, lanthanum oxide is added to the trifluoromethanesulfonic acid solution at a ratio of 10:1, heated to 80° C. under stirring conditions, reacted for 8 hours, filtered, and Remove the unreacted lanthanum oxide, concentrate the aqueous solution of lanthanum trifluoromethanesulfonate, and then place the concentrated aqueous solution of lanthanum trifluoromethanesulfonate at room temperature to naturally precipitate crystals, which is lanthanum trifluoromethanesulfonate with crystal water.

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Abstract

The invention provides a catalyst for polymerization of 1,3-pentadiene. The catalyst comprises a trifluoromethanesulfonic acid rare earth complex of which the chemical formula is Ln(CF3SO3)3.xH2O.yL and alkyl aluminum, wherein Ln is a tervalent cation of rare earth element; L is an electron-donating ligand; x is more than 0 and less than or equal to 6; and y is more than or equal to 1 and less than or equal to 4. The molar ratio of the alkyl aluminum to the Ln is (20-60):1. The catalyst can reduce preparation cost and simplify reaction conditions when poly-1,3-pentadiene is prepared; and prepared poly-1,3-pentadiene rubber has good performance. The invention also provides a preparation method for the catalyst for polymerization of the 1,3-pentadiene and a preparation method for the poly-1,3-pentadiene.

Description

technical field [0001] The invention relates to a catalyst and a preparation method thereof, and more to a preparation method of poly-1,3-pentadiene. Background technique [0002] 1,3-Pentadiene, also known as piperylene, is a conjugated diene that is second only to cyclopentadiene and isoprene in the C5 fraction of petroleum cracking. It is also relatively easy to obtain in the petrochemical industry A monomer that has not been used industrially so far. Poly-1,3-pentadiene rubber and its copolymer with butadiene have good physical and mechanical properties, and will become useful materials in the field of general-purpose synthetic rubber. Different catalytic systems can synthesize poly-1,3-pentadiene with different microstructures, such as cis-1,4, trans-1,4, syndiotactic-1,2, isotactic-1,2, no There are as many as 11 stereostructures such as 1, 2, 3, 4, etc., and the microstructure determines its physical and mechanical properties. Therefore, the research on homopolymeri...

Claims

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Application Information

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IPC IPC(8): C08F136/04C08F4/54C08F4/52C07F5/00
Inventor 代全权胡尊燕乔成莉蔡洪光张春雨张贺新毕吉福那丽华张学全
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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